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Process for making a germanium-zeolite. Atp MedicalLiterature - Series # 017. Source:http://www.sciencemag.org/cgi/content/full/304/5673/990

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characterizations of IM-

12, a thermally stablegermanium-containingzeolite . . . .)

Extra-Large-Pore Zeolites with Two-

Dimensional Channels Formed by14 and 12 RingsJean-Louis Paillaud,1* BogdanHarbuzaru,1 Jol Patarin,1 NicolasBats2

Stable zeolites that havelarger pore apertures and a three-dimensional pore topology are of

interest because they could be

used to adsorb largermolecules, particularly forapplication in oil

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refining.

Several large-pore zeoliticmaterials with channels formed byopenings of more than 12 rings areknown, but all of them have a one-dimensional channel system that

limits theiruse in catalysis.We report the synthesis and

some characterizations of IM-12, a

thermally stable

germanium-containingzeolite that contains the firsttwo-dimensional channel systemwith extra-large pores formed by 14-and 12-ring channels.

1 Laboratoire de MatriauxMinraux, UMR-CNRS 7016, EcoleNationale Suprieure de Chimie de

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Mulhouse, Universit de HauteAlsace, 3 rue Alfred Werner, 68093

Mulhouse Cedex, France.2 Institut Franais du Ptrole, IFP-Lyon, Bote Postale 3, 69390Vernaison, France.* To whom correspondence should

be addressed. E-mail:[email protected] of theirhigh

thermal stability, newzeolites are of interest inpetroleum refining, especially thosewith larger pores and systems ofintersecting channels that could
mailto:[email protected]:[email protected]


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potentially process

larger hydrocarbonmolecules. Two approacheshave led to larger pore systems.

One is the use offluoride

ions in place of OHspecies (13), because thefluoride appears to actas a structure-

directing agent (SDA)that plays a templating role (46).The other is the use of twosources of framework

atoms.For example, thesilicogermanates ITQ-12 (7), ITQ-17(8), ITQ-21 (9), and ITQ-22 (10)


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structures (13).Theoretical calculations

confirm this interpretation (14),together with the reportedpreferential occupation of thetetrahedral (T) sites of the D4R byGe in the zeolites obtained from Si-

and Ge-containing synthetic gels(1416), and also with the

observed fastercrystallization rate of

the ITQ-7 zeolite in itsSi- and Ge-containingform (14).

Scheme 1. One F-

containing D4Rcubic unit offormula T8O20, inwhich each T atom


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is at the center of atetrahedron and the

oxygen's atoms areat the vertices.[View LargerVersion of thisImage (32K GIFfile)]

We prepared the extra-largepore zeolite IM-12 (Institut Franais

du Ptrole/Mulhouse12), a Ge-containing zeolite, from afluoride-free synthesis medium inthe presence of organic (6R,10S)-6,10-dimethyl-5-azoniaspiro[4,5]decane cations as

SDA. This zeolitic materialdisplays a high
http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1


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thermal stability and

high adsorptioncapacity.

Depending on thecrystallization conditions (17), the

silicogermanate IM-12shows two differentcrystal morphologies.

Under static conditions,aggregates of size 150 by 150 by

200 m (Fig. 1A) resulting from thesuperposition ofthin platelet-like crystals areformed.

Under stirring conditions,gypsum flower-type


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aggregates are

produced with moreisolated crystals, withsizes of 5 by 5 m and thicknessesof about 300 nm (Fig. 1B).

The chemical and the thermal

gravimetric and differential thermalanalyses of IM-12synthesized in this wayindicated a Si/Ge

atomic ratio of about4.5 and a total weightloss of 15.7%, respectively,which are consistent with theunitcell formula: |(C11H22N)4(H2O;OH)16|


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reported for the microporoussilicogermanates with the topologies

ISV, ITH, and AST (1416,18).Thus, each layer is essentiallysiliceous and constructed of fusedsmall [415462] and [5262] cages.

The topology of IM-12 is that

of a 2D channel system formed by14- and 12-ring intersectingchannels parallel to the cand baxes, respectively (Fig. 2). The

framework density of

IM-12 is 15.2 T atomsper 1000 3.This value is lower than that of

other zeolitic materials containing14-ring channels, such as UTD-1

(19), CIT-5 (20), SSZ-53, and SSZ-59 (18,21) but higher than thoserecently reported for ECR-34 (18-ring pores) (22) and OSB-1 (a


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beryllosilicate with 14- and 8-ringintersecting channels) (18).

The crystallographic data ofIM-12 led to a free-pore diameter of9.5 by 7.1 and 8.5 by 5.5 for thestraight elliptical 14- and 12-ringchannels, respectively; these values

are comparable to 9.3 by 7.6 ,which was observed for the 14-ringopening of the borosilicate SSZ-59(21).

A calcination at

550C under air forseveral hours was sufficientto empty the pore volume of IM-12.Moreover, after several cycles ofcalcination at 600C, the structure of

IM-12 remained intact.We evaluated the


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adsorption capacity of

this highly thermally stable materialby N2adsorptionmeasurements. The N2adsorption isotherm of IM-12, of typeIa, according to the International

Union of Pure and AppliedChemistry nomenclature (fig. S2)

(17), is characteristic of amicroporous material

that lacks secondarymicropores andmesopores.

The corresponding

Brunauer-Emmet-Teller surface area of670 m2 g1 and the


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microporous volume of 0.26 cm3 g1

are similar to those of wellknown

highly porous zeolites oftopology FAU or EMT(18).

The pore-size distribution is

rather narrow and centered on 10 (fig. S3) (17). This value is slightlyhigher than the one calculated fromthe crystallographic data; thedisparity may reflect thenoncylindrical shape of the pores or

the effect of the side pockets of the12-ring channel, which the modeldoes not take into account (Fig. 3).

Fig. 2. The 3Dstructure and the

2D channel systemof the IM-12 zeolite.The connection


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between thesilicogermanate

layers lying in the(100) plane showsthe 14-ring channelalong [001] (left)and the 12-ringchannel along [010](right). The darkgray circles are theGe atoms. Thereare no openingsdown [100]. [View

Larger Version ofthis Image (60KGIF file)]

Fig. 3. View down a

direction close to[001] reveals thetie-shaped
http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3


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The ability to

incorporate Alsuggests that thismaterial may havecatalytic applicationsas well.References and Notes

1. E. M. Flaningen, R. L. Patton,U.S. Patent 4, 073, 865 (1978).

2. J.-L. Guth, H. Kessler, R. Wey,Stud. Surf. Sci. Catal.28, 121(1986).

3. J. Patarin, J.-L. Paillaud, H.Kessler, in Handbook of PorousSolids, F. Schth, K. S. W. Sing,

J. Weitkamp, Eds. (Wiley,Weinheim, Germany, 2002), vol.2, pp. 815876.

4. P. Caullet, J.-L. Guth, J.


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Hazm, J.-M. Lamblin, H. Gies,Eur. J. Solid State Inorg. Chem.

28, 345 (1991). 5. A. Corma, M. Puche, F. Rey,

G. Sankar, S. J. Teat,Angew.Chem. Int. Ed. Engl.42, 1156(2003).[Medline]

6. E. Aubert, F. Porcher, M.Souhassou, V. Petricek, C.Lecomte, J. Phys. Chem. B106,1110 (2002).[CrossRef]

7. P. A. Barrett et al., Chem.Commun.2003, 2114 (2003).[CrossRef]

8. A. Corma, M. T. Navarro, F.Rey, J. Rius, S. Valencia,Angew. Chem. Int. Ed. Engl.40,2277 (2001).[CrossRef][Medline]

9. A. Corma, M. J. Diaz-Cabanas, J. Martinez-Triguero,F. Rey, J. Rius, Nature418, 514
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(2002).[CrossRef][Medline] 10. A. Corma, F. Rey, S.

Valencia, J. L. Jorda, J. Rius,Nature Mater.2, 493 (2003).[CrossRef][ISI][Medline]

11. A. Corma, M. Navarro, F.Rey, S. Valencia, Chem.

Commun. 2001, 1486 (2001).[CrossRef] 12. A. Corma, M. J. Diaz-

Cabanas, F. Rey, Chem.Commun. 2003, 1050 (2003).[CrossRef]

13. M. O'Keeffe, O. M. Yaghi,Chem. Eur. J.5, 2796 (1999).[CrossRef]

14. T. Blasco et al., J. Phys.Chem. B106, 2634 (2002).

[CrossRef] 15. J. A. Vidal-Moya, T. Blasco,

F. Rey, A. Corma, M. Puche,
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Chem. Mater.15, 3921 (2003). 16. Y. Wang, J. Song, H. Gies,

Solid State Sci.5, 1421 (2003).[CrossRef]

17. Materials and methods areavailable as supporting materialon Science Online.

18. All framework type codes arederived from the names of thetype materials and consist ofthree capital Roman letters. Formore information, see Ch.Baerlocher, W. M. Meier, D. H.Olson,Atlas of ZeoliteFramework Types (Elsevier,Amsterdam, ed. 5, 2001); alsoavailable atwww.iza-structure.org/databases.

19. C. C. Freyhardt, M.Tsapatsis, R. F. Lobo, K. J.Balkus, M. E. Davis, Nature381,
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295 (1996).[CrossRef][ISI] 20. M. Yoshikawa et al., J. Phys.

Chem. B102, 7139 (1998).[CrossRef]

21. A. Burton et al., Chem. Eur.J.9, 5737 (2003).[CrossRef]

22. K. G. Strohmaier, D. E. W.

Vaughan, J. Am. Chem. Soc.125, 16035 (2003).[CrossRef][ISI][Medline]

23. We thank the InstitutFranais du Ptrole for providing

the germanium source. B.H.thanks the Ministre del'Education Nationale, de laRecherche et de la Technologiefor financial support.Supporting Online Material

www.sciencemag.org/cgi/content/full/304/5673/990/DC1

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